Cellulose ester film and its manufacturing method, optical film, polarizing plate and liquid crystal display

a technology of cellulose ester and manufacturing method, which is applied in the direction of instruments, polarizing elements, transportation and packaging, etc., can solve the problems of cellulose ester film, cellulose ester film, lowering transparency, etc., and achieves excellent flatness or appearance, excellent storage stability or productivity, and free

Active Publication Date: 2008-11-04
KONICA MINOLTA OPTO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0040]The microparticles in the invention is preferably microcapsules obtained by hydrolytic condensation of a reactive silicon compound. This method can adjust easily the relative standard deviation of the average primary particle diameter, exhibiting the effects of the invention. For example, there is a method disclosed in Japanese Patent Publication No. 5-4325 in which an alkoxysilane compound in the organic solution is hydrolytically condensed in the presence of excessive water, or a method disclosed in Japanese Patent No. 348461 in which an alkoxysilane compound in the gaseous phase is hydrolytically condensed in the presence of water droplets. There is, further, a method disclosed in Japanese Patent Publication No. 6-57317 in which microcapsules are dispersed in glycol, or a method disclosed in Japanese Patent No. 318752.
[0041]The cellulose ester film has a surface peak density of from 1,000 to 8,000 (1 / mm2), preferably from 2,000 to 6,000 (1 / mm2), and more preferably from 3,000 to 5,000 (1 / mm2). The above surface peak density range is preferred, since a greater surface peak density exhibits better sliding property, while a less surface peak density better transparency. The above surface peak density range can be obtained by adjusting the above average primary particle diameter of the microparticles and the above relative standard deviation of the particle diameter of the microcapsules. The microparticle content of the cellulose ester film of the invention is preferably from 0.02 to 1.0 g / m2, more preferably from 0.03 to 0.3 g / m2, and most preferably from 0.08 to 0.2 g / m2.
[0042]In the invention, the surface peak density is measured as follows: The number of peaks with a height of not less than 3 nm (preferably from 3 to 500 nm) on the film surface is measured at 23° C. and at a relative humidity RH of 50%+5% RH at an objective lens magnification of 50 and at an image zoom magnification of 1.0, employing a three dimensional surface structure analysis microscope zygo new View 5000 available from Canon Sales Co., Inc., and divided by an area measured to obtain the number per 1 mm2 of the peaks. In the invention, the surface peak density is represented in terms of the peak number per mm2 of the film.
[0043]In order to incorporate the microparticles in the invention into the cellulose ester film, an addition solution containing the microparticles is added to a dope as described later. A main dope to which the microparticles in powder are directly added results in insufficient dispersion, and a filter clogs with microparticle aggregates, resulting in rapid increase of filtration pressure. Therefore, it is preferred that a main dope, after added with the addition solution containing the microparticles, is filtered with for example, a filter capturing microparticles with a particle diameter of from 0.5 to 5 μm and giving a filtration time of from 10 to 25 sec / 100 ml. Incorporation of the addition solution containing the microparticles to the main dope may be any time before filtration as described above. The addition solution may be incorporated in the main dope placed in a dissolution vessel, or the main dope and the addition solution may be mixed in a mixing vessel provided separately. Before filtration, they may be mixed through a static mixer in a pipe leading to a filter. In most cases, the main dope contains return scraps in an amount of from 1.0 to 50% by weight. Since the return scraps contain microparticles, the content of the microparticles in the addition solution need to be adjusted depending upon the amount of the return scraps contained in the main dope. A method, in which the addition solution is added directly to the main dope and batch control is possible, or a method, in which the main dope and the addition solution are mixed in a mixing vessel, is preferred in view of ease of control. The former method is more preferred since time for mixing the main dope and the addition solution is sufficient and excellent productivity is obtained. The addition solution contains the microparticles in an amount of preferably from 0.5 to 10% by weight, more preferably from 1 to 5% by weight, and still more preferably from 1 to 3% by weight.
[0044]An addition solution having a low content of the microparticles is low in viscosity, which is easy to handle, while an addition solution having a high content of the microparticles can be added in a small amount to the main dope, which is easy to add. Therefore, the above microparticle content range is preferred. The return scraps herein referred to are cellulose ester pieces, for example, pieces produced by cutting the both edges of cellulose ester film web during manufacture, or cellulose ester film falling outside the specifications on account of scratches.
[0045]The main dope in the invention refers to a dope for manufacturing the cellulose ester film of the invention, and is distinguished from the addition solution. Resin, which the main dope contains in a high concentration, may be added in a small amount to the addition solution. In the invention, a dope containing most of film forming resin is referred to as the main dope, which is distinguished from the addition solution.

Problems solved by technology

However, such a film roll has problem in storage stability.
There is, for example, problem that the films are adhered to each other to deform or the films form a convex shape as if there is foreign matter between the films.
However, this method has problem in that when the amount of microparticles added to cellulose ester film is increased, it increases haze of the cellulose ester film, resulting in lowering of transparency.
It is difficult to obtain a cellulose ester film with improved sliding property and high transparency by increasing an amount of microparticles to be added to a cellulose ester film.
Therefore, there is problem in that the same Ra value may provide different effects in sliding property, haze or storage stability.

Method used

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  • Cellulose ester film and its manufacturing method, optical film, polarizing plate and liquid crystal display
  • Cellulose ester film and its manufacturing method, optical film, polarizing plate and liquid crystal display
  • Cellulose ester film and its manufacturing method, optical film, polarizing plate and liquid crystal display

Examples

Experimental program
Comparison scheme
Effect test

example 1

(Preparation of Silicon Oxide Addition Solutions “a” through “i”)

[0958]Cellulose acetate propionate (total acyl substitution degree of 2.65, an acetyl substitution degree of 1.90, and a propionyl substitution degree of 0.75) of 4.0 parts by weight were added to a mixture solvent of 82.6 parts by weight of ethylene chloride and 11.8 parts by weight of ethanol in a sealed vessel while stirring, and mixed while stirring employing a dissolver for 60 minutes. After that, 1.6 parts by weight of silicon oxide microparticles A through I as shown in Table 1 described later were added with stirring to the resulting mixture, and further stirred for 60 minutes. Thus, silicon oxide addition solutions “a” through “i” as shown in Table 2 were obtained. The average particle diameter of the particles in the silicon oxide addition solutions was measured through a particle size distribution meter LS 13320 series Multi Wave produced by Beckman-Coulter Co., Ltd.

[0959]The silicon oxide microparticles A t...

example 2

(Preparation of Cellulose Ester Film Samples 16 through 23)

(Main Dope C)

[0990]

Cellulose acetate89.5parts by weight(an acetylation degree of 60.9%)Triphenyl phosphate7.0parts by weightBiphenyl diphenyl phosphate3.5parts by weight

[0991]The above materials were dissolved in the following mixture solvent and stirred to obtain a dope with a solid concentration of 23.0% by weight.

[0992]

Methylene chloride82parts by weightMethanol15parts by weightn-Butanol3.0parts by weight

[0993]The resulting dope was filtered using a filter paper “#63” manufactured by Toyo Filter Paper Co. Ltd., further filtered using a sintered metal filter “06N” produced by Nippon Seisen Co., Ltd., and further filtered using a sintered metal filter “12N” (with a pore diameter of 40 μm) produced by Nippon Seisen Co., Ltd.

(Preparation of In-Line Addition Solution X)

[0994]

2(2′-Hydroxy-3′,5′-di-tert-5.40parts by weightbutylphenyl)-5-chlorobenzotriazole2(2′-Hydroxy-3′,5′-di-tert-10.79parts by weightamylphenyl)-5-chlorobenzotr...

example 3

[1016]The following antireflection layer solution was coated on the hard coat film samples 16 through 23 obtained above, to prepare hard coat film samples 16′ through 23′ with an anti-reflection layer.

>

[1017]

Titanium tetra-n-butoxide250parts by weightEnd group-reactive dimethylsilicone0.48parts by weightoil L-9000 produced by NipponUnicar Co., Ltd.)Aminopropyltrimethoxysilane KBE 90322parts by weight(produced by Shinetsu Kagaku Co., Ltd.)UV-curable epoxy resine21parts by weightKR 500 (produced by Asahi Denka Co., Ltd.)Propylene glycol monomethyl ether4900parts by weightIsopropyl alcohol4840parts by weight

[1018]

Titanium tetra-n-butoxide310parts by weightEnd group-reactive dimethylsilicone oil0.4parts by weightL-9000 produced by Nippon Unicar Co., Ltd.)Aminopropyltrimethoxysilane KBE 9034.8parts by weight(produced by Shinetsu Kagaku Co., Ltd.)UV-curable epoxy resine KR 5004.6parts by weight(produced by Asahi Denka Co., Ltd.)Propylene glycol monomethyl ether4900parts by weightIsopropyl...

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Abstract

Disclosed is a cellulose ester film containing cellulose ester and microparticles having an average primary particle diameter of from 0.1 to 1.0 μm, wherein a relative standard deviation of a primary particle diameter of the microparticles is from 1 to 20%, and wherein the cellulose ester film has a surface with a peak density of from 1,000 to 8,000 (1 / mm2).

Description

[0001]This application is based on Japanese Patent Application Nos. 2004-168647 filed on Jun. 7, 2004, and 2005-072201 fined on Mar. 15, 2005 in Japanese Patent Office, the entire content of which is hereby incorporated by reference.FIELD OF THE INVENTION[0002]The present invention relates to a cellulose ester film for optical use (hereinafter also referred to as a film) and its manufacturing method, and particularly to a cellulose ester film used in a polarizing plate protective film, a retardation film or a viewing angle increasing film for a liquid crystal display, in functional films for a plasma display such as an antireflection film, or in functional films for an organic EL display and its manufacturing method, and to an optical film, a polarizing plate and a liquid crystal display employing the cellulose ester film.BACKGROUND OF THE INVENTION[0003]Recently, study and development has been made regarding decrease in thickness and weight of a note board type personal computer, e...

Claims

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Application Information

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Patent Type & Authority Patents(United States)
IPC IPC(8): C09K19/02C09K19/52C08L1/10C08L1/12C09K19/00G02B1/10G02B5/30
CPCC08J5/18C08L1/10C08L1/12G02B1/105G02B5/3033Y10T428/1045C08J2301/12C08K5/3492Y10T428/1059Y10T428/1077Y10T428/1041Y10T428/10Y10T428/1036Y10T428/105C08J2301/10C09K2323/00C09K2323/03C09K2323/031C09K2323/033C09K2323/035C09K2323/05C09K2323/057G02B1/113G02B1/115G02B1/14G02B5/30G02F1/1335
Inventor MICHIHATA, ISAMU
Owner KONICA MINOLTA OPTO
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